Page No. 1/4
FC-PF-241
PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD,
NIPHM, HYDERABAD
Sr. No. in Scope
NABL / NON NABL
Flow Chart for Analysis of Methyl Parathion Dusting Powder Formulation
Date of Analysis
Sl. No.
1.
2.1
2.2
3.
Execution
Step
Sample No.
Name of Sample
Sample Description
Procedure
Preparation of Sample Solution
3.1
3.1.1
3.1.2
3.1.3
R2
R1
Weight of Sample taken equivalent to 0.8 g A.I in
250 mL Beaker
Purity of sample
Executed
By
g
g
%
%
Add 50 mL of Diethyl Ether and stir-well with a
glass rod.
Leave it to settle (3.1.3).
3.1.4
3.1.5
3.1.8
Filter (3.1.4) through sintered funnel with suction
pump.
Extract two more times with Ether, each time with
50 mL & all extracts filter through suction.
Collect the entire ether layer (3.1.6) into 500 mL
G.G.flask & evaporate on water bath to 2 mL.
Evaporate (3.1.7) completely at room temperature.
3.1.9
Add (3.1.8) 50 mL of Methanol.
3.1.10
Add (3.1.8) 25 mL of 1 N NaOH (aqueous).
3.1.11
3.1.12
Keep (3.1.8 to 3.1.10) for refluxion for 1 hour.
Cool (3.1.11) to room temperature. Rinse the
condenser with distilled water and remove the
flask.
Transfer it (3.1.12) into 1000 mL Volumetric Flask
quantitatively.
Make up to the mark with Distilled Water.
3.1.6
3.1.7
3.1.13
3.1.14
3.1.15
3.1.16
Pipette out 25 mL of above stock solution (3.1.14)
into a 250 mL volumetric flask.
Dilute up to the mark with Distilled Water.
3.1.17
Pipette out 10 mL of above stock solution (3.1.16)
Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow chart for analysis of Methyl Parathion in
Document No.
: FC-PF-241
Document Name
:
Dusting Powder.
Revision No.
: 01
Issue Date
:
01/06/2013
Revision Date
: 26/03/2014
Next Revision Date
:
26/03/2016
Prepared By
Checked By
Approved & Issued By
Mrs. C. Vijaya Lakshmi
(Assistant Plant Protection officer)
Mr. C.V. Rao
(Technical Manager)
Dr. Abhay Ekbote
(Director PM & Quality Manager)
Page No. 2/4
FC-PF-241
PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD,
NIPHM, HYDERABAD
3.1.18
3.1.19
3.1.20
3.1.21
3.2
into a 100 mL volumetric flask.
Dilute up to the mark with Distilled Water.
Switch on the UV-Visible Spectrophotometer & wait
for Stabilization.
Fill the Cuvettes with Distilled Water as a blank &
make the Instrument Absorbance to Zero.
Fill the Cuvettes with Sample solution (3.1.18) &
measure the absorbance at 400 nm.
Preparation of Standard Solution
3.2.2
Weigh 0.8 g of standard Technical Methyl Parathion
in 500 mL flat bottom G.G. flask.
Purity of Standard.
3.2.3
Add to it (3.2.1) 50 mL of Methanol.
3.2.4
Add to it (3.2.1) 25 mL of 1 N NaOH (aqueous).
3.2.5
Keep the mixture (3.2.4) for reflux for 1 hour & cool
to room temperature. After cooling wash the
condenser with distilled water, collect the washing
in the same receiver flask.
Transfer the contents into 1000 mL volumetric
flask & make up to the mark with Distilled Water.
Pipette out 25 mL of above stock solution (3.2.6)
into a 250 mL volumetric flask.
Dilute up to the mark with Distilled Water.
3.2.1
3.2.6
3.2.7
3.2.8
3.2.9
3.2.10
3.2.11
4.
4.1
4.2
5.
5.1
g
g
%
%
Pipette out 10 mL of above stock solution (3.2.8)
into a 100 mL volumetric flask.
Dilute up to the mark with Distilled Water.
Fill the Cuvettes with Standard solution (3.2.10) &
measure the absorbance at 400 nm in UV-Visible
Spectrophotometer.
Preparation of 1% Sodium Carbonate solution
Weigh about 5 g of Na2CO3 & dissolve in 500 mL
distilled water.
Make the above solution (4.1) into Chilled
condition.
Procedure for Impurities
Weight of Sample taken equivalent to 0.08 g A.I in
250 mL Beaker
Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow chart for analysis of Methyl Parathion in
Document No.
: FC-PF-241
Document Name
:
Dusting Powder.
Revision No.
: 01
Issue Date
:
01/06/2013
Revision Date
: 26/03/2014
Next Revision Date
:
26/03/2016
Prepared By
Checked By
Approved & Issued By
Mrs. C. Vijaya Lakshmi
(Assistant Plant Protection officer)
Mr. C.V. Rao
(Technical Manager)
Dr. Abhay Ekbote
(Director PM & Quality Manager)
Page No. 3/4
FC-PF-241
PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD,
NIPHM, HYDERABAD
5.2
5.3
5.4
5.5
5.6
5.7
5.8
5.9
5.10
5.11
5.12
5.13
5.14
5.15
5.16
Add 50 mL of Diethyl Ether and stir-well to
dissolve.
Leave it to settle (5.2).
Filter (5.3) through sintered funnel with suction
pump.
Extract the Pesticide into ether, for two more times,
each time with 50 mL ether & collect all the extracts
and filter through suction.
Collect the entire ether layer (5.5).
Transfer it (5.6) into 250 mL Separating funnel.
Extract free p-nitrophenol from (5.7) using 20 mL
each time with 1% chilled Sodium Carbonate
solution.
Collect the Yellow coloured aqueous layer into a
500 mL beaker.
Wash the contents in Separating funnel till Sodium
Carbonate layer becomes colourless and collect the
Yellow coloured layer.
Transfer the solution (5.9 & 5.10) into an
appropriate volumetric flask and make up to the
mark with distilled water.
Take the same quantity of Na2CO3 used in extraction
of impurities, into an appropriate volumetric flask.
Dilute the solution (5.12) up to the mark with
distilled water.
Use Na2CO3 solution for blank.
Fill the Cuvette with sample solution (5.13) and
measure the absorbance at 400 nm in UV-Visible
Spectrophotometer.
Record the absorbance.
6. Calculation:
Methyl Parathion content, % by mass =
[
A2 x M1
A1 x M2
]
xP
—
[
A3 x M1 x P
A1 x M3 x F
]
Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow chart for analysis of Methyl Parathion in
Document No.
: FC-PF-241
Document Name
:
Dusting Powder.
Revision No.
: 01
Issue Date
:
01/06/2013
Revision Date
: 26/03/2014
Next Revision Date
:
26/03/2016
Prepared By
Checked By
Approved & Issued By
Mrs. C. Vijaya Lakshmi
(Assistant Plant Protection officer)
Mr. C.V. Rao
(Technical Manager)
Dr. Abhay Ekbote
(Director PM & Quality Manager)
Page No. 4/4
FC-PF-241
PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD,
NIPHM, HYDERABAD
Where,
M1 =Mass in ‘g’ of Standard.
M2 = Mass in ‘g’ of Sample taken for test.
M3 = Mass in ‘g’ of Sample taken for p-nitrophenol (Impurities) extraction.
A1 = Absorbance of Standard solution.
A2 = Absorbance of Sample solution.
A3 = Absorbance of p-nitrophenol extract.
P = Percentage purity of Standard Methyl Parathion.
F = Dilution factor is 1000; if free p-nitrophenol is diluted to 100 mL.
400; if free p-nitrophenol is diluted to 250 mL.
200; if free p-nitrophenol is diluted to 500 mL.
Result:
Sl. No.
Name of test
1.
Methyl Parathion Content
Result
Unit
%
Remark / Reference :
Method of Analysis
IS 2570 : 1980
Reaffirmed 2007
Name
Analyzed by
Dated signature
Checked by
Name
Dated signature
Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow chart for analysis of Methyl Parathion in
Document No.
: FC-PF-241
Document Name
:
Dusting Powder.
Revision No.
: 01
Issue Date
:
01/06/2013
Revision Date
: 26/03/2014
Next Revision Date
:
26/03/2016
Prepared By
Checked By
Approved & Issued By
Mrs. C. Vijaya Lakshmi
(Assistant Plant Protection officer)
Mr. C.V. Rao
(Technical Manager)
Dr. Abhay Ekbote
(Director PM & Quality Manager)